Seals (psc-14)

ABSTRACT

A method, and the apparatus formed by encapsulating and stress forming a thermoplastic material upon a male member, e.g., the needle or plunger of a syringe, or both, to provide a durable and effective leak-proof seal when inserted within enclosing walls defining an opening of restricted diameter. A portion of the said male member is capped with an oversized thermoplastic material, the cap is then reduced in size to correspond to the diameter of the member with which it is to be mated in forming the seal, and then heated up to or just below the softening temperature of the thermoplastic material, generally up to about 425*F., and preferably to about 300*F. The heat stressed member, which is characterized as having very thin layers or films of the stress formed thermoplastic covering the external surface of the member, can then be inserted into snug fit within the mating bore, e.g., the barrel of a syringe, and the tight fit will endure because of the elastic memory of the material by virtue of which it tends to expand to its former size and shape thereby pressing against the enclosing side walls forming the bore.

Harris, Sr.

Inventor:

Assignee:

Filed:

Appl. No.: 66,136

SEALS (PSC-l4) Rano J. Harris, Sr., Baton Rouge, La.

Precision Sampling Corporation Aug. 21, 1970 Related US. Application Data [62] Division of Ser. No. 762,791, Sept. 26, 1968, Pat.

No. 3,577,850. I

[52] US. Cl. 222/386 [51] Int. Cl B67d 5/30 [58] Field of Search..... 222/386; 128/218 P, 218 C; 264/127, 230

[56] References Cited UNITED STATES PATENTS 2,895,773 7/1959 McConnaughey 128/218 P X 3,050,059 8/1962 Wall et a1. 128/218 P 3,147,753 9/1964 Nogier et 211.. 128/218 P 2,473,734 6/1949 Smith 128/218 P 3,537,453 11/1970 Drummond et'al.,. 128/218 C 2,608,334 8/1952 Knocke 264/230 X 3,290,946 12/1966 Pursell 222/386 X 3,619,478 11/1971 Staiger 264/230 3,634,924 l/l972 Blake et 31.... 264/230 3,093,526 6/1963 Price et a1 264/230 X 2,473,733 6/1949 Smith 128/218 P 3,577,850 5/1971 Harris, Jr. 222/386 Switzerland 128/218 P [451 Feb. 12,1974

386,164 12/1923 Germany.'. ..l28/218P 411,243 6/1966 Switzerland 128/218 P Primary Examiner-Samuel F. Coleman Assistant ExaminerNorman L. Stack, Jr. Attorney, Agent, or Firm-Llewellyn A. Proctor [5 7] ABSTRACT A method, and the apparatus formed by encapsulating and stress forming a thermoplastic material upon a male member, e.g., the needle or plunger of a syringe, or both, to provide a durable and effective leak-proof seal when inserted within enclosing walls defining an opening of restricted diameter. A portion of the said male member is capped with an oversized thermoplastic material, the cap is then reduced in size to correspond to the diameter of the member with which it is to be mated in forming the seal, and then heated up to or just below the softening temperature of the thermoplastic material, generally up to about 425F., and preferably to about 300F. The heat stressed member, which is characterized: as'having very thin layers or films'of the stress formed thermoplastic covering the external surface of the'member, can then be inserted into snug fit within the mating bore, e.g., the barrel of a syringe, and the tight fit will endure because of the elastic memory of the material by virtue of which it tends to expand to its former size and shape thereby pressing against the enclosing side walls forming the bore.

10 Claims, 3 Drawing Figures PAIENIEU FEB 1 21974 .SEAIQSCI14) This'is a division of application Ser. No. 762,791, filed Sept. 26, 1968, now US. Pat. No. 3,577,850.

In high accuracy, high precison prior art syringe constructions generally, the plunger and bore of the syringe barrel are precisely fitted. Both plunger and bore are generally round and free of taper to minimize interference, while yet allowing free movement of the plunger. The forward end or tip of the plunger is capped or covered with a suitable rubber or plastic material to form a movable seal. A ring of elastic material thus contacts the inside wall around the circumference of the barrel to provide sealing engagement. 'In this manner, escape of fluid around the annulus of the plunger is suppressed or prevented.

In such constructions also, a tubular needle is fitted upon the forward end of the barrel, and communicated with the bore thereof. Often the needle is cemented, packed, or sealed into the forward end of the barrel in fixed position to prevent or suppress leakage of fluid around the annulus of the needle.

Seals such as these and other types, whether fixed or movable, have proven generally satisfactory, but not so for high precision micro and semi-micro syringes, particularly where the fluid specimens, especially gas, must be handled at high temperatures, and withdrawn or injected against high pressures.

One difficulty with such seals is that the materials of which they are constructed all too rapidly lose their elasticity. Thus, even though a seal is sufficiently elastic ab initio to form a good snug fit, this condition does not endure. Often, the materials simply deteriorate, but even durable materials are known to cold flow. For example, the polytetrafluoroethylenes, e.g., Teflon, are known to form very good seals initially. Unfortunately, however, these materials cold flow and all too soon, e.g., the seal becomes loose so that leakage and inaccuracy result. In an effort to partially overcome this problem, e.g., plungers are often removed from the barrels and the plunger seals are heated in hot liquid, e.g., water, to produce expansion of the seal. The plunger is then placed in the syringe barrel for use in withdrawing and delivering a measured amount of a fluid specimen. This procedure is not only unsatisfactory in providing adequate sealing, but is quite burdensome. Such procedure is even less satisfactory, if at all feasible, when considered with respect to needle seals, or other fixed seals.

In recently issued US. Pat. No. 3,325,062, however, issued to a present inventor, syringes are described which have proven admirably suitable for the introduction of fluids, especially gases, into high pressure, high temperature systems. Such syringes are characterized, in part, by plungers, the forward ends of which are provided with gas filled seals, integral and movable with the plungers. The surface of the plungers are underscored, fitted with O-rings, covered with tightly fitting expandable or resilient caps, and then filled withgas sufficient to cause the outer surfaces of the caps to bulge outwardly to press tightly and snugly against the inside circumference of the barrel to form effective leak-proof seals. In this manner, fluids can be withdrawn or ejected from the syringes, even against high temperatures and pressures, without escape thereof around the annulus of the plunger.

While these seals have proven durable and eminently satisfactory, as well as having filled a long-felt need in the art, such seals are not generally satisfactory when the diameter of the plunger on which the seals are to be used is equal to or less then about 0.042 inch. Unfortunately, however, it is often necessary or desirable in high accuracy, high precision instrumentation to construct syringes with plunger diameters of 0.042 inch and less. Seals of these relatively small diameters become less and less effective as the diameters of the plungers are made smaller and smaller below this figure as is necessary for many micro and semi-micro measurements. Consequently, further improvements in plunger seals, especiallysmall diameter seals, are desired to serve the needs of industry. Moreover, improvements are needed in fixed seals to prevent leakage of fluid about the annuli of needles.

It is accordingly the primary objective of this invention to obviate the foregoing and other prior art deficiencies, and also fulfill the present needs.

In particular,'it is an object to provide highly accurate syringes adapted to measure and inject fluids at high precision, at relatively high temperature and pressures, directly into analytical devices without significant leakage. Y

Another object is to provide syringes, of micro and semi-micro capacities, with improved movable and fixed seals.

A further object is to provide new and novel stress formed seals, and as well a method for forming such seals.

These and other objects are achieved in accordance with the present invention by virtue of which new and' novel thermoplastic seals, of critical dimensions, are formed and shaped upon rigid members. The seals, when formed, are reduced in size and stressed so that when operatively positioned with enclosing walls defining a confined space, approximating that at which they were stressed, they constantly exert pressure against the enclosing walls sufficient to form a leak-proof seal due to a tendency to return to their original size.

Thermoplastic materials, of critical dimensions, can thus be snugly fitted over solid, sub-compact male members, e.g., syringe plungers and needles, or both, shaped, reduced in size, and, while restrained at the smaller size, heat-set at temperatures below the softening temperature of the thermoplastic materials. The thermoplastic material will thus possess a tendency to re-expand to its original larger diameter so that when positioned in an area of limited space, an outward thrust is exerted against a retaining wall. The soencapsulated end portion of a syringe plunger or needle will thus exert a thrust around the circumference of the internal barrel wall to form a leak-proof perpetually tight seal.

The present invention is based in part on the characteristics of various 'thermplastic organic materials which can be heat-set, resized and reshaped, at temperals. The polyfluoroethylenes, particularly polytetrafluoroethylene sold under the trake name Teflon, are also illustrative and, in fact, these self-lubricating plastics are particularly preferred materials used in the practice of the present invention. The desired temperature of setting varies with the specific nature of the material, and to some extent with time. In general, however, it is found that heat-setting is accomplished quite readily at temperature ranging up to about 425F. and preferably at temperatures ranging from about 200F. to about 300F.

The invention is also based in part on maintaining the heat stressed thermoplastic seal as a relatively thin skin or membrane, at the locations of contact with the enclosingv walls along which the sealing feature is provided. 7

These and other salient features and advantages of the invention are further and more fully described in the following detailed description which makes reference to the attached drawings:

Referring to the drawings:

FIG. 1 depicts an elevational view of a syringe, in partial section, provided with a needle and plunger with stress formed seals of type embodying the present invention;

FIG. 2 depicts graphically the process, or series of progressive steps (2a through 2e), employed from start to completion in shaping and stress forming a seal, e.g., a plunger seal; and

FIG. 3 depicts an enlarged view, taken on line 33 of FIG. 22, of a completed plunger, showing the critical dimensions of a seal embodying the present invention.

Referring to FIG. 1, there is shown a syringe formed by enclosing walls defining a tubular member or barrel 9. The barrel 9 is provided with an outwardly extending flange 16, and it is secured to the end of the barrel via threadable engagement with extension member which, likewise, can be threadably engaged, cemented or otherwise secured to the barrel.

The forward end of the barrel 9 is provided with a hollow or tubular needle 11, the rear portion of which is positioned through a shank or tip 12 and secured tightly therein to provide stability. The rear portion of the needle 11 is fitted snugly with a seal 13 which, in itself, is tightly fitted within the bore to prevent leakage of fluid about the needle annulus. The needle 11 is in open communication with the interior, or bore, of the barrel 9. Fluid can be withdrawn from a source (not shown) to enter the bore, and thereafter can be dispersed or ejected.

The barrel 9 is provided with a plunger 21 which is movable within the barrel. A handle or thumb-button facilitates the movement of the plunger 21 to withdraw or eject fluids from the barrel via passage through the needle 11. The plunger 21 is constructed, of any suitable material, e.g., stainless steel, spring wire or other resilient material, preferably metal. As heretofore suggested, the plunger diameters of micro and semi-micro syringes often range 0.042 inch and smaller.

Referring specifically to the plunger 21, it will be observed that the forward end thereof is encapsulated by a capping member 23 which, when shaped and heat-set in accordance with this invention, constantly seeks to expand to a larger diameter by virtue of an elastic memory" of its former larger size. The heat stressed capping member 23 is thus thrust circumferentially outwardly against the internal wall surface of the barrel 9 thereby effectively maintaining a snug and enduring fit, as well as sealing the annulus between the external surface of the plunger 21 and the internal wall surface of the barrel 9. It will also be observed that the needle 1 l is also provided with a stress formed seal 13, which can. be shaped and heat-set in accordance with the practice of this invention.

The concept of the general process of forming a tight and more enduring seal will be more fully appreciated by specific reference to FIGS. 2 and 3. These figures graphically depict the stress forming technique, and show as well certain critical dimensionswhich must be observed in forming such seals. While the figures show forming a seal on the forward end of a plunger, it is, of course, understood that the same technique is also applicable to other rigid members, e.g., a needle or other member, which necessitate, as a part of their function,

fixed or movable placement within enclosing walls defining a restriction or opening.

The sequence of five figuresviz., 2a through 2eshows generally the capping of the forward end of a plunger, the shaping and encapsulation of the forward end, completion of the stress forming within a mold and its removal therefrom as a completed plunger ready for use by insertion in a syringe barrel.

In referring to the sequence described by reference to FIG. 2, there is shown a die or mold 20 provided with an internal opening sized to correspond in diameter with that of the bore of the barrel in which the finished plunger is to be used. It is to be understood, of course, that a seal can be formed in situ within the bore of the syringe or other device within which it is to be used.

The forward end of the plunger 21 is roughened, anodized, or underscored more preferably by one or a plurality of circumferential grooves 22. The function of the groove 22 is to provide a non-smooth surface for retention of an open centered thermoplastic cap 23, after insertion of the forward end of the plunger therein as shown by reference to FIGS. 2a and 2b.

The thermoplastic cap 23, it will be observed, is initially of larger diameter than the axial opening of the die or mold 20. As the plunger 21 is thrust forward, as shown by reference to FIGS. 21:, 2c and 2d, the cap 23 is brought into contact with the enlarged frusto conic shaped opening 19, and as the forward movement of the plunger 21 is continued, the cap 23 enters the axial opening and is reduced in diameter; ultimately to the diameter of axial opening. As the reduction in size of cap 23 progresses, the excess thermoplastic material is initially rejected and gradually forced backward to cover the whole forward end of the plunger, which is of slightly less diameter than that of the axial opening. Eventually, the thermoplastic material fills virtually the whole, or nearly the whole, of the volume of the recessed portion 24 of the plunger.

In a preferred syringe combination, a plunger is thus provided with a recessed portionwhich trails the forward end of the plunger. The recessed portion is sufficiently large to retain the excess thermoplastic material as the diameter of the initial capping member is reduced to the desired dimension. Preferably, the recessed portion provides a volume substantially equal to, or almost equal to, the volume of the thermoplastic material displaced. The forward end of the completed plunger will be provided with a surface of thermoplastic material, and the sum-total diameter of the encapsulated forward end will thus be equal to, or almost equal to, the diameter of the non-encapsulated portion of the plunger.

Once the entire encapsulated forward end of the plunger is contained within the axial opening, the thermoplastic material is heat-set by raising the temperature of the mold up to or just below the softening temperature of the material of which cap 23 is composed. As heretofore suggested, temperatures ranging up to about 425F., and preferably from about 200F. to about 300F., are sufficient. Of course, the mold 20 can be preheated to the desired temperature prior to insertion of the plunger.

Upon withdrawal of the plunger 21, as shown by reference to FIG. 2e, the stress forming and formation of the seal is completed. The plungerZl, with its soformed seal, is now ready for insertion into the barrel or bore of a syringe l0, e.g., as shown by reference to FIG. 1. As indicated heretofore, a seal 13 can be formed for needle 11, or any male member, in similar fashion.

In the completed seals, it is absolutely essential that the thickness of the skin or membrane of stress formed thermoplastic material which contacts the surrounding walls of an opening be relatively thin. Thus, with reference to FIG. 3, the single thickness d of the encapsulating film formed on rigid members of diameter ranging from about 0.025 inch to about 0.042 inch should range from about 0.001 inch to no greater than about 0.005 inch. Thicknesses ranging from about 0.0015 inch to about 0.0025 inch are most preferred. Seals constructed .in accordance with such requirements have been found to fit quite tightly for indefinite periods of time without becoming loose. In fact, such seals actually become a little tighter as time passes. Consequently, the seals are quite durable and remain virtually leak-proof even when subjected to high temperaturehigh pressure service. Teflon seals formed in accordance with these requirements, e.g., have provided outstanding service and the normal cold flow associated with this material has had little effect, if any, in lessening tight fits.

The relative thinness of the layers of stress formed thermoplastic material between the male member, or plunger, and the enclosing wall is a key and novel feature in providing the enduring tight fit. It is essential. Thick layers will not accomplish this result, even when the layers are of stress formed thermoplastic materials. This is because the thin layers are less affected by loss of elasticity and cold flow than the thicker layers. This can be conveniently explained by assuming a given percent loss of elasticity over a period of time for a specific stress formed thermoplastic material, e.g., 2 percent loss over a given interval of time. One can thus readily visualize the effect of a 2 percent loss of elasticity in a 0.001 inch membrane as compared, e.g., with a membrane of 0.1 inch thickness. The adverse effect of a two percent loss in elasticity will thus have a one hundred times greater effect on the latter than on the former. Considerably less force will be exerted against an enclosing wall by the thicker membrane. Such loss of force will hardly be measurable, however, in the thinner membrane. Hence, the thicker membane is entirely ineffective in providing an enduring tight fit as is sharply contrasted with the thinner membrane.

EXAMPLE By way of illustration, a micro syringe was formed utilizing, in formation of the plunger, an 0.018 inch outside diameter stainless steel wire. The forward end of the plunger was roughened and grooved by etching with a file. The outside diameter of the wire forming the forward end of the plunger was reduced to between about 0.0l20.0l3 inch, and a recessed portion was provided just behind the forward now enlarged end. The relatively large forward end of the plunger, about three thirty-seconds inch in length, was then partially covered with a 0.026 inch outside diameter Teflon cap having an opening about 0.012 inch inside diameter, and one-sixteenth inch in depth. The plunger was pressed into a bore having an internal diameter of 0.019 inch, and heated to 300F.

It was found that the stress formed Teflon encapsulated plunger could be used in the bore of the syringe, which had an inside diameter of 0.019 inch, to provide an enduring leak-proof seal. The seal was capable of withstanding relatively high pressures and temperatures in withdrawing and delivering fluids, even gases, with high accuracy and precision.

EXAMPLE 2 When a syringe having a bore of 0.042 inch internal diameter was formed from a stainless steel wire initially 0.032 inch in diameter in similar manner to provide stress formed layers, a single thickness of which was 0.005 inch, a high durability leak-proof seal was again obtained. Gas, at high accuracy and precision, was delivered by the syringe to a G.C. column against a pressure of 500 psig.

It is apparent that various modifications and changes can be made without departing the spirit and scope of the invention. 1

Having described the invention, what is claimed is:

1. In combination, apparatus defined by an enclosing wall forming a tubular barrel, a reciprocable plunger of substantially uniform outside diameter fitted snugly within the bore of the barrel, a thermoplastic material, encapsulating the forward end of the plunger, heat stressed at a temperature below the melting point of said thermoplastic material, and reduced in thickness from a former greater thickness to a thickness ranging from about 0.001 inch to no greater than about 0.005 inch, the sum-total diameter of the plunger inclusive of the total thickness of the heat stressed themioplastic material ranges up to about 0.042 inch, and the said thermoplastic material fits tightly and enduringly within the bore to form an effective leak-proof seal about the annulus of the plunger.

2. The apparatus of claim 1 wherein the tubular barrel is the barrel portion of a needle syringe, and the needle at the forward end of the barrel at the location wherein it is fitted onto the barrel is also provided with a similar heat stressed seal which prevents leakage about the annulus of the needle.

3. In apparatus constituting a small diameter male member, a portion thereof of which is of reduced diameter to provide a retention surface for an encapsulating thermoplastic covering material which, when pressed within enclosing walls defining a restricted opening of substantially corresponding diameter, forms an effective leak-proof seal the improvement which comprises providing a male member, inclusive of the thickness of the encapsulating covering thermoplastic mate rial, of no greater than about 0.042 inch in diameter, and an encapsulating thermoplastic material of thickness ranging from about 0.001 to about 0.005 inch, said thermoplastic material having been reduced to said thickness from a material of greater thickness and heat set under stress at the'reduced thickness at a temperature just below the softening temperature of the thermoplastic material, and said heat stressed thermoplastic material fits tightly and enduringly within the enclosing walls to form an effective leak-proof seal.

4. The apparatus of claim 3 wherein the thickness of the encapsulating heat set thermoplastic material ranges from about 0.0015 to about 0.0025 inch.

5. The apparatus of claim 3 wherein the diameter of the male member, inclusive of the thickness of the thermoplastic material, ranges from about 0.025 to about 0.042 inch.

6. The apparatus of claim 3 wherein the thermoplastic material is Teflon.

7. The apparatus of claim 3 wherein the male member is a needle of a micro syringe.

8. The apparatus of claim 3 wherein the male mem- 

1. In combination, apparatus defined by an enclosing wall forming a tubular barrel, a reciprocable plunger of substantially uniform outside diameter fitted snugly within the bore of the barrel, a thermoplastic material, encapsulating the forward end of the plunger, heat stressed at a temperature below the melting point of said thermoplastic material, and reduced in thickness from a former greater thickness to a thickness ranging from about 0.001 inch to no greater than about 0.005 inch, the sum-total diameter of the plunger inclusive of the total thickness of the heat stressed thermoplastic material ranges up to about 0.042 inch, and the said thermoplastic material fits tightly and enduringly within the bore to form an effective leak-proof seal about the annulus of the plunger.
 2. The apparatus of claim 1 wherein the tubular barrel is the barrel portion of a needle syringe, and the needle at the forward end of the barrel at the location wherein it is fitted onto the barrel is also provided with a similar heat stressed seal which prevents leakage about the annulus of the needle.
 3. In apparatus constituting a small diameter male member, a portion thereof of which is of reduced diameter to provide a retention surface for an encapsulating thermoplastic covering material which, when pressed within enclosing walls defining a restricted opening of substantially corresponding diameter, forms an effective leak-proof seal the improvement which comprises providing a male member, inclusive of the thickness of the encapsulating covering thermoplastic material, of no greater than about 0.042 inch in diameter, and an encapsulating thermoplastic material of thickness ranging from about 0.001 to about 0.005 inch, said thermoplastic material having been reduced to said thickness from a material of greater thickness and heat set under stress at the reduced thickness at a temperature just below the softening temperature of the thermoplastic material, and said heat stressed thermoplastic material fits tightly and enduringly within the enclosing walls to form an effective leak-proof seal.
 4. The apparatus of claim 3 wherein the thickness of the encapsulating heat set thermoplastic material ranges from about 0.0015 to about 0.0025 inch.
 5. The apparatus of claim 3 wherein the diameter of the male member, inclusive of the thickness of the thermoplastic material, ranges from about 0.025 to about 0.042 inch.
 6. The apparatus of claim 3 wherein the thermoplastic material is Teflon.
 7. The apparatus of claim 3 wherein the male member is a needle of a micro syringe.
 8. The apparatus of claim 3 wherein the male member is a plunger of a micro syringe.
 9. The apparatus of claim 3 wherein the encapsulating thermo-plastic material has a history of having been heat-treated at temperatures ranging up to about 425*F.
 10. The apparatus of claim 9 wherein the history of heat treat-ment was conducted at temperatures ranging from about 200*F. to about 300*F. 